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Title

Implementation of a generic liquid chromatographic methoddevelopment workflow: Application to the analysis ofphytocannabinoids and Cannabis sativa extracts

Authors
Molnar, Imre
Published in Journal of Pharmaceutical and Biomedical Analysis. 2018, vol. 155, p. 116-124
Abstract A generic liquid chromatographic method development workflow was developed and successfullyapplied to the analysis of phytocannabinoids and Cannabis sativa extracts. Our method developmentprocedure consists in four steps:i) The screening of primary parameters (i.e. stationary phase nature, organic modifier nature and approx-imate mobile phase pH) was carried out with a generic gradient on a short narrow bore column, using asystem able to accommodate numerous solvents/buffers and columns. Instead of complete peak track-ing, the number of peaks which can be separated was considered as a response at this level, to savetime.ii) The optimization of secondary parameters (i.e. gradient conditions, mobile phase temperature and pHwithin a narrow range) requires only 12 initial experiments and the use of HPLC modeling software fordata treatment. It allows to find out the best retention and selectivity for the selected compounds. Peaktracking was performed with a single quadruple mass detector in single ion recording mode, and UVdetection (in a broad wavelength range).iii) The refinement step allows to further adjust column efficiency, by tuning column length and mobilephase flow rate. This can also be done virtually using HPLC modeling software.iv) The robustness testing step was also evaluated from a virtual experimental design. Success rate andregression coefficients were estimated in about 1 min, without the need to perform any real experiment.At the end, this method development workflow was performed in less than 4 days and minimizes thecosts of the method development in liquid chromatography.
Keywords CannabinoidsCannabisMethod developmentRobustness testDryLabUHPLC
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Research group Sciences analytiques
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FEKETE, Szabolcs et al. Implementation of a generic liquid chromatographic methoddevelopment workflow: Application to the analysis ofphytocannabinoids and Cannabis sativa extracts. In: Journal of Pharmaceutical and Biomedical Analysis, 2018, vol. 155, p. 116-124. https://archive-ouverte.unige.ch/unige:103447

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Deposited on : 2018-04-10

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